Potassium Hydroxide → HCID 19738531, Verbindung
Reaktionsgleichung
[CH3:1][O:2][CH:3]([O:11][CH3:12])[CH2:4][NH:5][C:6](=[O:10])[O:7][CH2:8][CH3:9].[OH-].[K+].[Cl:15][C:16](=[CH2:19])[CH2:17]I>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.C1(C)C=CC=CC=1>[Cl:15][C:16](=[CH2:17])[CH2:19][N:5]([CH2:4][CH:3]([O:2][CH3:1])[O:11][CH3:12])[C:6](=[O:10])[O:7][CH2:8][CH3:9]Komponenten
Versuchsvorschrift
115 g (0.65 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate, 130 g of powdered potassium hydroxide and 2 g of triethylbenzylammonium chloride are initially introduced into 650 ml of toluene and 142 g (0.7 mol) of 2-chloroallyl iodide are added dropwise at room temperature. After stirring overnight, a gas chromatogram showed incomplete conversion, hence 65 g of powdered potassium hydroxide and 1 g of triethylbenzylammonium chloride were added again and a further 71 g (0.35 mol) of 2-chloroallyl iodide were added dropwise. After stirring overnight at room temperature, the salts were filtered off with suction, the filtrate was washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated, and the residue was distilled.
Aufarbeitung
- additionare added dropwise at room temperature
- additionwere added again
- stirringAfter stirring overnight at room temperature
- filtrationthe salts were filtered off with suction
- washthe filtrate was washed with saturated sodium chloride solution
- dry with materialdried over magnesium sulphate
- concentrationconcentrated
- distillationthe residue was distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-5629be5ac52940e49115953ee0106d35
- Quelldatensatz
- uspto-grants-1993_01
- Patentnummer
- US05177210
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